تفاعل #343840

معادلة التفاعل

calcium oxide

6-chloro-7-[(4-fluorophenyl)methyl]-8-[[1-(phenylmethyl)-4-piperidinyl]-methyl]-7H-purine

hydrogen

→

7-[(4-fluorophenyl)methyl]-8-(4-piperidinylmethyl)-7H-purine

المردود 54.0%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe catalyst was filtered off
2. 2
   أخرىthe filtrate was evaporated
3. 3
   استخلاصThe product was extracted with dichloromethane
4. 4
   أخرىThe extract was dried
5. 5
   ترشيحfiltered
6. 6
   أخرىevaporated
7. 7
   أخرىThe residue was purified by column chromatography over silica gel using
8. 8
   workup.ADDITIONa mixture of trichloromethane and methanol
9. 9
   أخرىThe pure fractions were collected
10. 10
    أخرىthe eluent was evaporated

الإجراء التجريبي

A mixture of 15 parts of 6-chloro-7-[(4-fluorophenyl)methyl]-8-[[1-(phenylmethyl)-4-piperidinyl]-methyl]-7H-purine. 5 parts of calcium oxide and 200 parts of methanol was hydrogenated at normal pressure and at room temperature with 2 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The residue was taken up in water. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia. (95:5→85:15 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 5.8 parts (54%) of 7-[(4-fluorophenyl)methyl]-8-(4-piperidinylmethyl)-7H-purine as a residue (compound 55).

المصدر